Modified phosphorus-nitrogen type flame retardant and preparation method thereof
A flame retardant and modification technology, which is applied in the field of modified phosphorus-nitrogen flame retardant and its preparation, can solve the problems of easy blooming, easy migration, poor compatibility, etc., and achieve the effect of good dispersion and difficult agglomeration
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Embodiment 1
[0028] A modified phosphorus nitrogen type flame retardant, made by the following method:
[0029] Step S1. Add pentaerythritol into a three-necked flask, place it in an ice-water bath, stir at a speed of 100r / min for 30min, add phosphorus oxychloride dropwise while stirring, control the dropping time to 15min, and use a mass fraction of 20% during the dropping process. % sodium hydroxide aqueous solution to absorb the tail gas, stir at a constant speed for 30 minutes after the dropwise addition, then raise the temperature to 60°C, stir at a constant speed at this temperature for 2 hours, heat up to 100°C, reflux until no hydrogen chloride is produced, cool and filter with suction after the reaction , the filter cake was washed three times with chloroform and absolute ethanol, and then transferred to a vacuum drying oven with a vacuum degree of -0.10 MPa, and dried at 50°C for 10 hours to obtain the first product. In step S1, pentaerythritol and three The weight ratio of phosp...
Embodiment 2
[0036] A modified phosphorus nitrogen type flame retardant, made by the following method:
[0037] Step S1. Add pentaerythritol into a three-necked flask, place it in an ice-water bath, stir at a speed of 100r / min for 30min, add phosphorus oxychloride dropwise while stirring, control the dropping time to 15min, and use a mass fraction of 20% during the dropping process. % sodium hydroxide aqueous solution to absorb the tail gas, stir at a constant speed for 30 minutes after the dropwise addition, then raise the temperature to 60°C, stir at a constant speed at this temperature for 2 hours, heat up to 100°C, reflux until no hydrogen chloride is produced, cool and filter with suction after the reaction , the filter cake was washed three times with chloroform and absolute ethanol, and then transferred to a vacuum drying oven with a vacuum degree of -0.10 MPa, and dried at 50°C for 10 hours to obtain the first product. In step S1, pentaerythritol and three The weight ratio of phosp...
Embodiment 3
[0044] A modified phosphorus nitrogen type flame retardant, made by the following method:
[0045] Step S1. Add pentaerythritol into a three-necked flask, place it in an ice-water bath, stir at a speed of 100r / min for 30min, add phosphorus oxychloride dropwise while stirring, control the dropping time to 15min, and use a mass fraction of 20% during the dropping process. % sodium hydroxide aqueous solution to absorb the tail gas, stir at a constant speed for 30 minutes after the dropwise addition, then raise the temperature to 60°C, stir at a constant speed at this temperature for 2 hours, heat up to 100°C, reflux until no hydrogen chloride is produced, cool and filter with suction after the reaction , the filter cake was washed three times with chloroform and absolute ethanol, and then transferred to a vacuum drying oven with a vacuum degree of -0.10 MPa, and dried at 50°C for 10 hours to obtain the first product. In step S1, pentaerythritol and three The weight ratio of phosp...
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